JP Food Sanitation Law "Positive List" for Pesticide Residue

FUJIFILM Wako offers over 1100 standard products ((certified reference material (CRM), single standards and standard mixture solutions)) for the "positive list" in Japan. Our CRM and standard products are highly purified based on our purification technology. The purity of almost all products is determined by qNMR. The high-quality standard products are essential for making chromatographic measurements and their assured values are important for final analytical results. qNMR using reference standards with traceability to the International System of Units (SI) recently attracts attention as one of absolute purity determining methods for standards for chromatography, because of its efficiency and reliability. In fact, qNMR has been used as the official analytical method regarding the Japanese Pharmacopoeia, Japanese Standards for Food Additives, and the Japanese Industrial Standard. We started to establish a supply system for standard products with absolute purity values determined by qNMR. We explored an appropriate framework for sample preparation procedures, NMR parameter sets, sample distribution ways and selection of target signal(s) of each compound. As a result, we found that qNMR was able to determine the purity of normal small molecular organic compounds with the accuracy of less than or equal to 1%. We established a supply system for standard products of very high purity such as pesticides, catechins, amino acids, natural toxins (e.g. mycotoxin), dietary supplements, and functional compounds.

PPL1-PPL5

Pesticide Mixture Standard Solution PL-1-2 (each 20μg/ml Acetone Solution)

GC/MS Chromatogram*

00370_img03.png
Peak No. Constituent Monitoring Ions (m/z) Peak No. Constituent Monitoring Ions (m/z) Peak No. Constituent Monitoring Ions (m/z)
1 Omethoate 156 110 141 11 Malathion (Malathon) 173 158   21 Pyrethrin I, II 123 133 162
107 133 160
2 Trifluralin 306 264   12 Fenpropimorph 128 129 303 22 Norflurazon 145 303 173
3 Dimethoate 87 125   13 Pendimethalin 252 281   23 Diflufenican 266 394
4 Atrazine 200 215   14 Penconazole 159 248   24 Bifenthrin 181 166
5 Terbufos 231 288 153 15 Procymidone 283 285   25 Azinphos-methyl 160 132
6 Tefluthrin 177 197 383 16 Methidathion (DMTP) 145 85 302 26 Fenarimol 139 330 251
7 Spiroxamine 100 126 17 Fenamiphos 303 217 27 trans-Permethirn 183 163
100 101 126
8 Chlorpyrifosmethyl 286 288 18 Oxadiazon 175 302 344 28 cis-Permethirn 183 163
9 Terbutryn 226 241 19 Kresoxim-methyl 116 206 29 Cyfluthrin 163 226 206
10 Thiobencarb (Benthiocarb) 100 257 20 Chlorfenapyr 364 328 30 Flucythrinate 199 451
31 Fluvalinate 250 252
  • *Analysis conditions, charts, and detected ions are reference data. It is not the data to guarantee the pesticide mixed standard solution.

Analysis conditions

[ Instrument ]

Shimadzu QP-2010 Ultra

[GC]

Column Rtx-5MS 0.25 μm, 0.32 mm×30 m

Column temperature 80 ℃ (1 min)→20 ℃/min→180 ℃→5 ℃/min→300 ℃ (10 min)

Injection temperature 260 ℃

Carrier gas He 2.2 mL/min

Splitless 1 min

[MS]

Ionization EI

Interface temperature 280 ℃

Pesticide Mixture Standard Solution PL-2-1 (each 20μg/ml Acetone Solution)

GC/MS Chromatogram*

00370_img04.png
Peak No. Constituent Monitoring Ions (m/z) Peak No. Constituent Monitoring Ions (m/z) Peak No. Constituent Monitoring Ions (m/z)
1 Propoxur (PHC) 110 152   11 Isofenphos Oxon 229 314   21 Propiconazole 173 259  
2 Carbofuran 164 149   12 Chlorfenvinphos(α-CVP, β-CVP) 267 323   22 Hexazinone 171 252 128
3 Quintozene (PCNB) 237 295   13 Isofenphos 213 255   23 Propargite (BPPS) 173 150
4 Propyzamide 173 255   14 Triadimenol 112 168   24 Phosmet (PMP) 160 161 133
5 Tri-allate 268 128   15 Tetrachlorvinphos (CVMP) 329 331   25 Methoxychlor 227 274 228
6 Vinclozolin 285 212   16 Isoprothiolane 118 290   26 Pyriproxyfen 136 226  
7 Alachlor 160 188   17 Myclobutanil 179 150   27 Pyraclofos 360 194  
8 Fenitrothion (MEP) 277 260   18 Buprofezin 105 172   28 Fluquinconazole 340 108  
9 Metolachlor 162 238   19 Cyproconazole 222 139   29 Fenbuconazole 129 198  
10 Fenthion (MPP) 278 169   20 Ethion 231 384   30 Fluridone 328 329  
31 Difenoconazole 323 265
  • *Analysis conditions, charts, and detected ions are reference data. It is not the data to guarantee the pesticide mixed standard solution.

Analysis conditions

[ Instrument ]

Shimadzu QP-2010 Ultra

[GC]

Column Rtx-5MS 0.25 μm, 0.32 mm×30 m

Column temperature 80 ℃ (1 min)→20 ℃/min→180 ℃→5 ℃/min→300 ℃ (10 min)

Injection temperature 260 ℃

Carrier gas He 2.2 mL/min

Splitless 1 min

[MS]

Ionization EI

Interface temperature 280 ℃

Pesticide Mixture Standard Solution PL-3-3 (each 20μg/ml Acetone Solution)

GC/MS Chromatogram*

00370_img05.png
Peak No. Constituent Monitoring Ions (m/z) Peak No. Constituent Monitoring Ions (m/z) Peak No. Constituent Monitoring Ions (m/z)
1 Ethoprophos 158 200 139 11 Fipronil 367 369 351 21 Fenpropathrin 181 265 349
2 Simazine (CAT) 201 173 12 Flutolanil 173 323 22 Cyhalothrin 181 197 208
3 Diazinon 137 152 304 13 Profenofos 139 337 374 23 Bitertanol 170 168 112
4 Propanil (DCPA) 161 217 14 Oxyfluorfen 252 361 300 24 Pyridaben 147 309
5 Parathion-methyl (Methylparathion) 125 233 263 15 Chlorobenzilate 139 251 25 Cypermethrin 163 181 165
6 Pirimiphos-methyl 290 276 305 16 Triazophos 161 257 26 Fenvalerate 125 419 225
7 Chlorpyrifos 197 286 314 17 Quinoxyfen 237 272 307 27 Deltamethrin 181 253
8 Parathion 291 235 18 Tebuconazole 125 250
9 Triadimefon 208 181 19 Acetamiprid 166 221
10 Allethrin 123 136 20 Bromopropylate (Phenisobromolate) 341 183
  • *Analysis conditions, charts, and detected ions are reference data. It is not the data to guarantee the pesticide mixed standard solution.

Analysis conditions

[ Instrument ]

Shimadzu QP-2010 Ultra

[GC]

Column Rtx-5MS 0.25 μm, 0.32 mm×30 m

Column temperature 80 ℃ (1 min)→20 ℃/min→180 ℃→5 ℃/min→300 ℃ (10 min)

Injection temperature 260 ℃

Carrier gas He 2.2 mL/min

Splitless 1 min

[MS]

Ionization EI

Interface temperature 280 ℃

Pesticide Mixture Standard Solution PL-4-2 (each 20μg/ml Acetone Solution)

GC/MS Chromatogram*

00370_img06.png
Peak No. Constituent Monitoring Ions (m/z) Peak No. Constituent Monitoring Ions (m/z) Peak No. Constituent Monitoring Ions (m/z)
1 Mevinphos
( (E)-Mevinphos,
(Z)-Mevinphos
)
127 109 192 13 Chlorthal-dimethyl (TCTP) 301 299 332 25 Fluacrypyrim 145 320 189
2 Tecnazene 203 215 261 14 Fthalide 243 241 272 26 Lenacil 153 154 110
3 Ethalfluralin 276 316 15 Fosthiazate 139 166 283 27 (E)-Pyriminobac-methyl 302 256 303
4 Monocrotophos 127 192 16 Dimepiperate 119 145 28 Mefenpyr‐diethyl 253 255 299
5 Dicloran (CNA) 206 208 176 17 Phenthoate (PAP) 274 246 29 Pyridaphenthion 340 199 188
6 Pyroquilon 173 130 172 18 Butachlor 176 237 30 Etoxazole 141 359 300
7 Phosphamidon 264 193 19 Imazamethabenz Methyl (Imazamethabenz-methyl) 144 245 256 31 Anilofos 125 334 184
8 δ-BHC 181 183 219 20 Uniconazole P 234 236 32 Tetradifon 159 229 356
9 Dimethenamid 154 230 203 21 Pretilachlor 162 238 262 33 Mefenacet 192 120
10 Tolclofos-methyl 265 267 125 22 Azaconazole 217 173 219 34 Halfenprox 263 265 183
11 Ametryn 227 212 23 Bupirimate 273 208 316 35 Tralomethrin** 181 253
12 Diethofencarb 225 267 24 (Z)-Pyriminobac-methyl 302 256 303 36 Imibenconazole 253 375
  • *Analysis conditions, charts, and detected ions are reference data. It is not the data to guarantee the pesticide mixed standard solution.
  • **Peak No. 35 is detected as Deltamethrin.

Analysis conditions

[ Instrument ]

Shimadzu QP-2010 Ultra

[GC]

Column Rtx-5MS 0.25 μm, 0.32 mm×30 m

Column temperature 80 ℃ (1 min)→20 ℃/min→180 ℃→5 ℃/min→300 ℃ (10 min)

Injection temperature 260 ℃

Carrier gas He 2.2 mL/min

Splitless 1 min

[MS]

Ionization EI

Interface temperature 280 ℃

Pesticide Mixture Standard Solution PL-5-1 (each 20μg/ml Acetone Solution)

GC/MS Chromatogram*

00370_img07.png
Peak No. Constituent Monitoring Ions (m/z) Peak No. Constituent Monitoring Ions (m/z) Peak No. Constituent Monitoring Ions (m/z)
1 Isoprocarb (MIPC) 121 136 13 (Z)-Dimethylvinphos 295 297 25 Fensulfothion 293 308
2 Propachlor 120 176 14 Tetraconazole 336 338 26 Mepronil 119 269 133
3 Chloropropham (Chloro IPC) 127 171 213 15 Bromophos 331 329 27 Benalaxyl 148 206 228
4 Cadusafos 159 158 114 16 Dimethametryn 212 255 71 28 Pyraflufen-ethyl 412 414 349
5 Pyrimethanil 198 199 17 Diclocymet 277 221 29 Thenylchlor 127 288 141
6 Terbacil 161 160 117 8 (E)-Pyrifenox 262 294 264 30 Zoxamide 187 189 258
187 242
7 Iprobenfos (IBP) 204 246 19 Fenothiocarb 72 160 31 EPN 157 169 185
8 Benfuresate 163 121 256 20 Prothiofos 309 267 32 Bifenox 341 343 310
9 Acetochlor 146 162 223 21 Tricyclazole 189 118 33 Phosalone 182 121 367
10 Simetryne 213 155 170 22 Tribufos 169 202 34 Acrinathrin 181 289 208
11 Prometryn 241 184 226 23 Imibenconazole-debenzyl 235 270 128 35 Etofenprox 163 135
12 Esprocarb 222 162 24 Isoxathion 177 313 36 Flumiclorac‐pentyl 423 353 308
37 Fluthiacet-methyl 403 405
  • *Analysis conditions, charts, and detected ions are reference data. It is not the data to guarantee the pesticide mixed standard solution.

Analysis conditions

[ Instrument ]

Shimadzu QP-2010 Ultra

[GC]

Column Rtx-5MS 0.25 μm, 0.32 mm×30 m

Column temperature 80 ℃ (1 min)→20 ℃/min→180 ℃→5 ℃/min→300 ℃ (10 min)

Injection temperature 260 ℃

Carrier gas He 2.2 mL/min

Splitless 1 min

[MS]

Ionization EI

Interface temperature 280 ℃

PPL6-PPL10

Pesticide Mixture Standard Solution PL-6-3 (each 20μg/ml Acetone Solution)

GC/MS Chromatogram*

00370_img08.png
Peak No. Constituent Monitoring Ions (m/z) Peak No. Constituent Monitoring Ions (m/z) Peak No. Constituent Monitoring Ions (m/z) Peak No. Constituent Monitoring Ions (m/z)
1 XMC 122 107   11 Quinoclamine (ACN) 172 209   21 Flamprop‐methyl 105 276   31 Cyhalofop-butyl 256 357 229
2 Benfluralin (Bethrodine) 292 264 276 12 Cyanazine 225 240 198 22 Fenoxanil 189 293 328 32 Pyrazophos 221 232 373
3 Propazine 214 229 172 13 Nitrothal‐isopropyl 236 194 254 23 Oxadixyl 163 132 233 33 Cafenstrole 100 188
4 Cyanophos (CYAP) 109 243 125 14 Diphenamid 167 239 165 24 Edifenphos (EDDP) 173 201 310 34 Flumioxazin 354 287 355
5 Prohydrojasmon 153 184 15 (Z)-Pyrifenox 262 294 264 25 Trifloxystrobin 116 131 222 35 Tolfenpyrad 383 385   
6 Benoxacor 120 259 176 16 Quinalphos 146 157 298 26 Diclofop‐methyl 340 253 281           
7 Dichlofenthion (ECP) 279 223 162 17 Paclobutrazol 236 238 138 27 Pyributicarb 165 108 181           
8 Bromobutide 119 232    18 Napropamide 128 100   28 Piperophos 122 140             
9 Mefenoxam (Metalaxyl M) 206 249 234 19 Butamifos 286 200   29 Tebufenpyrad 318 276 333           
10 Bromacil 205 190   20 Hexaconazole 214 216 231 30 Phenothrin 123 183             
  • *Analysis conditions, charts, and detected ions are reference data. It is not the data to guarantee the pesticide mixed standard solution.

Analysis conditions

[ Instrument ]

Shimadzu QP-2010

[GC]

Column Rtx-5MS 0.25 μm, 0.32 mm×30 m

Column temperature 80 ℃ (1 min)→20 ℃/min→180 ℃→5 ℃/min→300 ℃ (10 min)

Injection temperature 260 ℃

Carrier gas He 2.2 mL/min

Splitless 1 min

[MS]

Ionization EI

Interface temperature 280 ℃

Pesticide Mixture Standard Solution PL-7-2 (each 20μg/ml Acetonitrile Solution)

LC/MS/MS Chromatogram*

00370_img09.png
Peak No. Constituent Monitoring Ions (m/z) Mode Peak No. Constituent Monitoring Ions (m/z) Mode Peak No. Constituent Monitoring Ions (m/z) Mode
Precursor Product Precursor Product Precursor Product
1 Thiamethoxam 292.2 210.9 + 11 (E)-Ferimzone 255.2 91.1 + 21 Fenoxycarb 302.3 116.0 +
2 Clothianidin 250.2 131.9 + 12 (Z)-Ferimzone 255.2 91.1 + 22 Anilofos 368.2 124.9 +
3 Chloridazon (PAC) 222.2 104.0 + 13 Methoxyphenozide 369.2 149.0 + 23 Cyflufenamid 413.1 295.0 +
4 Thiacloprid 253.1 126.0 + 14 Iprovalicarb 321.2 119.1 + 24 Pyrazolynate (Pyrazolate) 439.0 172.9 +
5 Thiabendazole 202.2 175.0 + 15 Chromafenozide 395.4 175.0 + 25 Indoxacarb (Indoxacarb-MP) 528.2 150.0 +
6 Azamethiphos 325.0 182.9 + 16 Butafenacil 492.1 330.9 + 26 Benzofenap 431.1 105.0 +
7 Dimethirimol 210.2 71.1 + 17 Simeconazole 294.2 70.0 + 27 Furathiocarb 383.2 195.0 +
8 Isoxaflutole 360.1 250.9 + 18 Oryzalin 347.1 304.9 + 28 Cloquintocet-mexyl 336.3 237.9 +
9 Azinphos-methyl 318.0 132.1 + 19 Cyazofamid 325.0 108.0 + 29 Abamectin B1a (Abamectin) 890.6 305.2 +
10 Pyriftalid 319.1 139.0 + 20 Naproanilide 292.2 171.0 +
  • *Analysis conditions, charts, and detected ions are reference data. It is not the data to guarantee the pesticide mixed standard solution.

Analysis conditions

[ Instrument ]

Shimadzu LCMS-8040

[HPLC]

Column Wakopak® Wakosil-Ⅱ 3C18HG 2.0 × 150 mm

Column temperature 40 ℃

Eluent A) 5 mmol/L CH3COONH4 in H2O, B) 5 mmol/L CH3COONH4 in CH3OH

Gradient

Time (min) B conc. (%)
0-1 15-40
1-3.5 40
3.5-6 40-50
6-8 50-55
8-17.5 55-95
17.5-30 95
30-40 95-15

Flow rate 0.2 mL/min

[MS]

Ionization ESI

Mode MRM

Pesticide Mixture Standard Solution PL-8-1 (each 20μg/mL Acetonitrile Solution)

LC/MS/MS Chromatogram*

00370_img10.png
Peak No. Constituent Monitoring Ions (m/z) Mode Peak No. Constituent Monitoring Ions (m/z) Mode
Precursor Product Precursor Product
1 Flumetsulam 326.2 128.9 + 12 1-Naphthaleneacetic Acid 185.2 141.2
2 Thifensulfuron-methyl 388.2 167.0 + 13 Cloprop 199.2 127.1
3 Florasuram 360.1 128.9 + 14 Ioxynil 369.8 127.0
4 Cloransulam-methyl
(Cloransulam methyl)
430.2 397.9 + 15 Triclopyr 253.9 196.1
5 Diclosulam 406.0 160.9 + 16 Mecoprop (MCPP) 213.1 141.1
6 Thidiazuron 221.1 102.0 + 17 Dichlorprop 233.0 161.1
7 Forchlorfenuron 248.1 128.9 + 18 MCPB 227.1 141.1
8 Gibberellin (Gibberellin A3) 345.1 143.2 19 Acifluorfen 360.2 316.2
9 Fluroxypyr 253.0 195.0 20 Fomesafen 436.9 195.2
10 4-Chlorophenoxyacetic Acid
(4-CPA)
185.2 127.1 21 Haloxyfop 356.0 288.2
11 Bromoxynil 275.9 81.0               
  • *Analysis conditions, charts, and detected ions are reference data. It is not the data to guarantee the pesticide mixed standard solution.

Analysis conditions

[ Instrument ]

Shimadzu LCMS-8040

[HPLC]

Column Wakopak® Wakosil-Ⅱ 3C18HG 2.0 ×150 mm

Column temperature 40 ℃

Eluent A) 5 mmol/L CH3COONH4 in H2O, B) 5 mmol/L CH3COONH4 in CH3OH

Gradient

Time (min) B conc. (%)
0-1 15-40
1-3.5 40
3.5-6 40-50
6-8 50-55
8-17.5 55-95
17.5-30 95
30-40 95-15

Flow rate 0.2 mL/min

[MS]

Ionization ESI

Mode MRM

Pesticide Mixture Standard Solution PL-9-2 (each 20μg/ml Acetone Solution)

GC/MS Chromatogram*

00370_img11.png
Peak No. Constituent Monitoring Ions (m/z) Peak No. Constituent Monitoring Ions (m/z)
1 EPTC 128 132 189 10 Famphur 218 217 125
2 Etridiazole (Echlomezol) 211 183 246 11 Endosulfan Sulfate (Benzoepin Sulfate) 272 387 422
3 Chloroneb 191 193 206 12 Piperonyl Butoxide 176 177   
4 Fenobucarb (BPMC) 121 150    13 Bioresmethrin 123 171 143
5 Diphenylamine 169 168 167 14 Iprodione 314 316   
6 Propetamphos 138 236 194 15 Iprodione Metabolite 329 331   
7 Pirimicarb 166 238   16 Fenoxaprop-ethyl 288 361 261
8 Imazalil 215 217 173 17 Prochloraz 180 308 266
9 Flusilazole 233 206 315               
  • *Analysis conditions, charts, and detected ions are reference data. It is not the data to guarantee the pesticide mixed standard solution.

Analysis conditions

[ Instrument ]

Shimadzu QP-2010

[GC]

Column Rtx-5MS 0.25 μm, 0.32 mm×30 m

Column temperature 80 ℃ (1 min)→20 ℃/min→180 ℃→5 ℃/min→300 ℃ (10 min)

Injection temperature 260 ℃

Carrier gas He 2.2 mL/min

Splitless 1 min

[MS]

Ionization EI

Interface temperature 280 ℃

Pesticide Mixture Standard Solution PL-10-1 (each 20μg/ml Acetone Solution)

GC/MS Chromatogram*

00370_img12R.png
Peak No. Constituent Monitoring Ions (m/z) Peak No. Constituent Monitoring Ions (m/z)
1 Aldicarb(deg.) 68 115 100 6 Carbaryl (NAC) 144 115 116
2 Aldoxycarb (Aldicarb sulfone) (deg.) 68 80     7 Metalaxyl 206 249   
3 Acephate 136 94     8 Thiabendazole 201 174   
4 Bendiocarb 151 166 223 9 Azoxystrobin 344 388   
5 Metribuzin 198 144                  
  • *Analysis conditions, charts, and detected ions are reference data. It is not the data to guarantee the pesticide mixed standard solution.

Analysis conditions

[ Instrument ]

Shimadzu QP-2010 Ultra

[GC]

Column Rtx-5MS 0.25 μm, 0.32 mm×30 m

Column temperature 50 ℃ (1 min)→20 ℃/min→180 ℃→5 ℃/min→300 ℃ (10 min)

Injection temperature 260 ℃

Carrier gas He 2.3 mL/min

Splitless 1 min

[MS]

Ionization EI

Interface temperature 280 ℃

PPL11-PPL15

Pesticide Mixture Solution PL-11-2 in Hexane 20 ug/ml

GC/MS Chromatogram*

00370_img13.png
Peak No. Constituent Monitoring Ions (m/z) Peak No. Constituent Monitoring Ions (m/z)
1 Hexachlorobenzene 286 249   9 cis-Chlordane (α-Chlordane) 375 272   
2 Heptachlor 337 274   10 Dieldrin 277 261   
3 Aldrin 265 261 293 11 p,p'-DDE 318   
4 Dicofol(Kelthane) (deg.) [DCBP] 250 12 Endrin 317 345 245
5 Heptachlor Epoxide (isomer A) 351 13 p,p'-DDD 237 165
6 Oxychlordane 389 14 o,p'-DDT 237 165
7 Heptachlor Epoxide (isomer B) 351 15 p,p'-DDT 237 165 212
8 trans-Chlordane (γ-Chlordane) 375 272
  • *Analysis conditions, charts, and detected ions are reference data. It is not the data to guarantee the pesticide mixed standard solution.

Analysis conditions

[ Instrument ]

Shimadzu QP-2010

[GC]

Column Rtx-5MS 0.25 μm, 0.32 mm × 30 m

Column temperature 50 ℃ (1 min)→20 ℃/min→180 ℃→5 ℃/min→300 ℃ (10 min)

Injection temperature 260 ℃

Carrier gas He 2.2 mL/min

[MS]

Ionization EI

Interface temperature 280 ℃

Pesticide Mixture Standard Solution PL-12-1 (each 20μg/ml Acetone Solution)

GC/MS Chromatogram*

00370_img14.png
Peak No. Constituent Monitoring Ions (m/z) Peak No. Constituent Monitoring Ions (m/z) Peak No. Constituent Monitoring Ions (m/z)
1 Chlorethoxyfos 153 263 11 Mecarbam 111 153 21 Carfentrazone-ethyl 312 340 330
2 Dicrotophos 127 193 237 12 Methoprene 131 159 22 Epoxiconazole 192 138 165
3 Phorate 75 121 260 13 Bromophos-ethyl 359 303 23 Picolinafen 376 238
4 Clomazone 125 204 14 Propaphos 220 304 24 Fenamidone 238 268
5 Isazofos 161 257 172 15 Chlorbenside 125 127 268 25 Spirodiclofen 312 259
6 Disulfoton (Ethylthiomethon) 88 274 16 Flutriafol 123 164 219 26 Cinidon-ethyl 330 358
7 Formothion 125 125 17 Chlorofenson (CPCBS) 111 175 302
8 Fenchlorphos 285 287 18 Carboxin 143 235            
9 Ethofumesate 207 161 286 19 1,1-Dichloro-2,2-bis (4-ethylphenyl) ethane 223 224 167           
10 2-(1-Naphthyl) acetamide(1-Naphthylacetamide) 141 185     20 Flufenpyr-ethyl 408 335              
  • *Analysis conditions, charts, and detected ions are reference data. It is not the data to guarantee the pesticide mixed standard solution.

Analysis conditions

[ Instrument ]

Shimadzu QP-2010

[GC]

Column BPX5 0.25 μm, 0.32 mm×30 m

Column temperature 80 ℃ (1 min)→20 ℃/min→180 ℃→5 ℃/min→300 ℃ (5 min)

Injection temperature 260 ℃

Carrier gas He 2.2 mL/min

Splitless 1 min

[MS]

Ionization EI

Interface temperature 280 ℃

Pesticide Mixture Standard Solution PL-13-1 (each 20μg/ml Acetone Solution)

GC/MS Chromatogram*

00370_img15.png
Peak No. Constituent Monitoring Ions (m/z) Peak No. Constituent Monitoring Ions (m/z)
1 Nitrapyrin 194 196     9 Resmethrin 123 171    
2 Methacrifos 208 180 240 10 Furathiocarb 163 194   
3 Tebuthiuron 156 171    11 Triticonazole 235 237 299
4 Oxabetrinil 73 77 103 12 Boscalid 140 342 344
5 S-Metolachlor 162 238    13 Thiacloprid 251 101   
6 Flufenacet 151 211    14 Famoxadone 330 196 197
7 Triflumizole 206 278    15 Propaquizafop 443 299   
8 Azamethiphos 215 217 324               
  • *Analysis conditions, charts, and detected ions are reference data. It is not the data to guarantee the pesticide mixed standard solution.

Analysis conditions

[ Instrument ]

Shimadzu QP-2010 Ultra

[GC]

Column BPX5 0.25 μm, 0.32 mm×30 m

Column temperature 80 ℃ (1 min)→20 ℃/min→180 ℃→5 ℃/min→300 ℃ (5 min)

Injection temperature 260 ℃

Carrier gas He 2.2 mL/min

Splitless 1 min

[MS]

Ionization EI

Interface temperature 280 ℃

Pesticide Mixture Standard Solution PL-14-2 (each 20μg/ml Acetonitrile Solution)

LC/MS/MS Chromatogram*

00370_img16.png
Peak No. Constituent Monitoring Ions (m/z) Mode Peak No. Constituent Monitoring Ions (m/z) Mode Peak No. Constituent Monitoring Ions (m/z) Mode
Precursor Product Precursor Product Precursor Product
1 Methomyl 163.1 88.0 + 11 Acibenzolar-S-methyl 211.0 135.9 + 21 Pencycuron 329.2 125.0 +
2 Imidacloprid 256.1 175.0 + 12 Dymron (Daimuron) 269.2 151.0 + 22 Hexaflumuron 463.1 157.9 +
3 Oxycarboxin 268.1 174.9 + 13 Cumyluron 303.2 185.0 + 23 Cycloate 216.2 83.1 +
4 Bendiocarb 224.3 109.0 + 14 Chloroxuron 291.1 72.1 + 24 Pentoxazone 354.1 286.1 +
5 Thiodicarb 355.1 87.9 + 15 Mepanipyrim 224.3 106.0 + 25 Oxaziclomefone 376.1 190.0 +
6 Pirimicarb 239.2 72.0 + 16 Triticonazole 318.3 70.0 + 26 Fenoxaprop-ethyl 362.1 287.9 +
7 Methabenzthiazuron 222.1 165.0 + 17 Indanofan 341.1 175.0 + 27 Flufenoxuron 489.0 158.0 +
8 Furametpyr 334.1 156.9 + 18 Tetrachlorvinphos (CVMP) 366.9 127.0 + 28 Cycloprothrin 499.1 180.9 +
9 Azoxystrobin 404.1 372.0 + 19 Carpropamid 336.1 138.9 + 29 Spinosad** (Spinosyn A) 732.4 142.1 +
10 Methiocarb 226.1 169.0 + 20 Imazalil 297.1 158.9 + (Spinosyn D) 746.6 142.0 +
30 Silafluofen 426.2 287.0 +
  • *Analysis conditions, charts, and detected ions are reference data. It is not the data to guarantee the pesticide mixed standard solution.
  • **The preparation concentration is converted to 20 µg/mL as a total of Spinosyn A and Spinosyn D.

Analysis conditions

[ Instrument ]

Shimadzu LCMS-8040

[HPLC]

Column Wakopak® Wakosil-Ⅱ 3C18HG 2.0 × 150 mm

Column temperature 40 ℃

Eluent A) 5 mmol/L CH3COONH4 in H2O, B) 5 mmol/L CH3COONH4 in CH3OH

Gradient

Time (min) B conc. (%)
0-1 15-40
1-3.5 40
3.5-6 40-50
6-8 50-55
8-17.5 55-95
17.5-30 95
30-40 95-15

Flow rate 0.2 mL/min

[MS]

Ionization ESI

Mode MRM

Pesticide Mixture Standard Solution PL-15-1 (each 20μg/mL Acetonitrile Solution)

LC/MS/MS Chromatogram*

00370_img17.png
Peak No. Constituent Monitoring Ions (m/z) Mode Peak No. Constituent Monitoring Ions (m/z) Mode Peak No. Constituent Monitoring Ions (m/z) Mode
Precursor Product Precursor Product Precursor Product
1 Aldoxycarb
(Aldicarb sulfone)
240.0 86.1 + 11 Fenamidone 312.0 92.2 + 21 (Z)-Fenpyroximate 422.1 366.2 +
2 Oxamyl 237.0 72.0 + 12 Flufenacet 364.0 152.1 + 22 Hexythiazox 354.1 229.1 +
3 Aldicarb 208.0 116.1 + 13 Epoxiconazole 331.1 121.1 + 23 (E)-Fenpyroximate 422.1 366.2 +
4 Carbofuran 222.1 165.1 + 14 Diflubenzuron 328.0 158.2 + 24 Diuron (DCMU) 232.0 186.9
5 Tebuthiuron 229.1 172.3 + 15 Tebufenozide 353.1 297.2 + 25 Linuron 247.9 160.7
6 Carbaryl (NAC) 202.0 145.1 + 16 Cyprodinil 226.1 93.1 + 26 Boscalid 342.9 113.9
7 Monolinuron 215.1 126.2 + 17 Triflumuron 359.1 156.2 + 27 Novaluron 491.1 84.6
8 Fluridone 330.0 309.1 + 18 Clofentezine 304.0 138.1 + 28 Teflubenzuron 381.1 152.1
9 (E)-Dimetomorph** 389.0 302.1 + 19 Quizalofop-ethyl 373.1 299.0 + 29 Lufenuron 508.9 339.1
10 (Z)-Dimetomorph** 389.0 302.1 + 20 Propaquizafop 445.1 100.1 +          
  • *Analysis conditions, charts, and detected ions are reference data. It is not the data to guarantee the pesticide mixed standard solution.
  • **The preparation concentration is converted to 20 µg/mL as a total of E and Z isomers.

Analysis conditions

[ Instrument ]

Shimadzu LCMS-8040

[HPLC]

Column Wakopak® Wakosil-Ⅱ 3C18HG 2.0 × 150 mm

Column temperature 40 ℃

Eluent A) 5 mmol/L CH3COONH4 in H2O, B) 5 mmol/L CH3COONH4 in CH3OH

Gradient

Time (min) B conc. (%)
0-1 15-40
1-3.5 40
3.5-6 40-50
6-8 50-55
8-17.5 55-95
17.5-30 95
30-30.01 95-15
30.01-40 15

Flow rate 0.2 mL/min

[MS]

Ionization ESI

Mode MRM

PPL16-PPL17

Pesticide Mixture Standard Solution PL-16-2 (each 20μg/mL Acetonitrile Solution)

LC/MS/MS Chromatogram*

00370_img18.png
Peak No. Constituent Monitoring Ions (m/z) Mode Peak No. Constituent Monitoring Ions (m/z) Mode Peak No. Constituent Monitoring Ions (m/z) Mode
Precursor Product Precursor Product Precursor Product
1 Metsulfuron-methyl 382.1 167.0 + 11 Pyrazosulfuron-ethyl 415.1 182.0 + 21 Fluazifop 328.1 282.1 +
2 Azimsulfuron 425.1 182.0 + 12 Naptalam 292.1 144.0 + 22 Triflusulfuron-methyl 493.1 264.1 +
3 Cinosulfuron 414.1 183.0 + 13 Trifloxysulfuron 438.1 182.0 + 23 Bensulfuron-methyl 411.1 149.1 +
4 Sulfosulfuron 471.1 211.0 + 14 Iodosulfuron-methyl 508.1 166.9 + 24 Primisulfuron-methyl 469.0 254.0 +
5 Flazasulfuron 408.1 182.0 + 15 Metosulam 418.0 174.9 + 25 Cyclosulfamuron 422.1 217.9 +
6 Imazosulfuron 413.1 156.0 + 16 Penoxsulam 484.1 195.0 + 26 Fenhexamid 302.1 97.1 +
7 Propoxycarbazone** 399.1 199.0 + 17 Chlorimuron-ethyl 415.1 186.0 + 27 Halosulfuron-methyl 433.1 252.0
8 Triasulfuron 402.1 167.0 + 18 Ethoxysulfuron 399.1 261.0 + 28 2,4-D (2,4-PA) 218.9 161.0
9 Mesosulfuron-methyl 504.1 182.0 + 19 Prosulfuron 420.1 141.0 + 29 MCPA (MCP) 198.9 141.0
10 Ethametsulfuron-methyl 411.1 196.0 + 20 Clodinafop Acid 312.0 266.0 + 30 Sulfentrazone 384.9 307.0
  • *Analysis conditions, charts, and detected ions are reference data. It is not the data to guarantee the pesticide mixed standard solution.
  • **The preparation concentration is converted to 20 µg/mL as a free base.

Analysis conditions

[ Instrument ]

Shimadzu LCMS-8040

[HPLC]

Column Wakopak® Wakosil-Ⅱ 3C18HG 2.0 × 150 mm

Column temperature 40 ℃

Eluent A) 5 mmol/L CH3COONH4 in H2O, B) 5 mmol/L CH3COONH4 in CH3OH

Gradient

Time (min) B conc. (%)
0-1 25-40
1-3.5 40
3.5-6 40-50
6-8 50-55
8-17.5 55-95
17.5-30 95
30 -40 95-25

Flow rate 0.2 mL/min

[MS]

Ionization ESI

Mode MRM

Pesticide Mixture Standard Solution PL-17-2 (each 20μg/ml Acetonitrile Solution)

LC/MS/MS Chromatogram*

00370_img19.png
Peak No. Constituent Monitoring Ions (m/z) Mode Peak No. Constituent Monitoring Ions (m/z) Mode Peak No. Constituent Monitoring Ions (m/z) Mode
Precursor Product Precursor Product Precursor Product
1 Pymetrozine 218.1 105.1 + 11 Flamprop-methyl 336.1 105.1 + 21 Trifloxystrobin 409.1 186.1 +
2 3-OH Carbofuran (3-Hydroxycarbofuran) 255.1 163.1 + 12 Triflumizole Metabolite 295.1 73.1 + 22 Triflumizole 346.1 73.1 +
3 Cymoxanil 199.2 128.1 + 13 Prometryn 242.4 200.1 + 23 Benfuracarb 411.3 195.1 +
4 Carbetamide 237.2 188.1 + 14 Clodinafop-propargyl 350.1 266.1 + 24 Fluazuron 506.1 158.0 +
5 Bromacil 261.0 205.0 + 15 Carfentrazone-ethyl 411.5 365.5 + 25 Etoxazole 360.2 141.0 +
6 Oxabetrinil 233.1 87.1 + 16 Benalaxyl 326.1 148.1 + 26 Chlorfluazuron 540.1 383.0 +
7 Chlorbufam 224.1 172.0 + 17 Mefenpyr-diethyl 373.2 327.0 + 27 Amitraz 294.2 163.1 +
8 Ametryn 228.1 186.1 + 18 Pyraclostrobin 390.1 194.1 + 28 Carbosulfan 381.2 118.1 +
9 Pyrimethanil 200.1 107.1 + 19 Phoxim 299.1 129.1 + 29 Fenpropimorph 304.2 147.1 +
10 Barban 275.2 177.9 + 20 Pyrazophos 374.2 222.1 +          
  • *Analysis conditions, charts, and detected ions are reference data. It is not the data to guarantee the pesticide mixed standard solution.

Analysis conditions

[ Instrument ]

Shimadzu LCMS-8040

[HPLC]

Column Wakopak® Wakosil-Ⅱ 3C18HG 2.0 × 150 mm

Column temperature 40 ℃

Eluent A) 5 mmol/L CH3COONH4 in H2O, B) 5 mmol/L CH3COONH4 in CH3OH

Gradient

Time (min) B conc. (%)
0-1 15-40
1-3.5 40
3.5-6 40-50
6-8 50-55
8-17.5 55-95
17.5-30 95
30 -40 95-15

Flow rate 0.2 mL/min

[MS]

Ionization ESI

Mode MRM

VPL1-VPL2

Veterinary Drug Mixture Standard Solution PL-1-3 (each 20μg/ml Methanol Solution)

LC/MS/MS Chromatogram*

00370_img20.png
Peak No. Constituent Monitoring Ions (m/z) Mode Peak No. Constituent Monitoring Ions (m/z) Mode
Precursor Product Precursor Product
1 Lincomycin** 407.2 126.2 + 12 Dexamethasone 393.2 337.0 +
2 Sulfacetamide 215.1 155.9 + 13 Emamectin B1a 887.6 158.1 +
3 Danofloxacin** 358.2 82.0 + 14 Famphur 326.1 92.8 +
4 Clenbuterol ** 277.1 203.0 + 15 Fenobucarb (BPMC) 208.2 95.0 +
5 Xylazine ** 221.3 90.0 + 16 Temephos (Abate) 467.0 124.9 +
6 Pyrimethamine 249.1 176.9 + 17 Allethrin 303.2 135.1 +
7 Trichlorfon (DEP) 257.1 108.8 + 18 Monensin 688.4 125.1 +
8 Tilmicosin 869.5 174.0 + 19 Florfenicol 358.1 185.1
9

Tiamulin**

494.3 192.1 + 20 2-Acetylamino-5-nitro thiazole 186.2 139.1
10 Prednisolone 361.2 147.0 + 21 Clorsulon 380.0 344.0
11 Hydrocortisone 363.3 121.0 +               
  • *Analysis conditions, charts, and detected ions are reference data. It is not the data to guarantee the pesticide mixed standard solution.
  • **The preparation concentration is converted to 20 µg/mL as a free base.

Analysis conditions

[ Instrument ]

Shimadzu LCMS-8040

[HPLC]

Column Wakopak® Wakosil-Ⅱ 3C18HG 3.0 × 150 mm

Column temperature 40 ℃

Eluent A) 0.1% HCOOH in H2O, B) 0.1% HCOOH in CH3CN

Gradient

Time (min) B conc. (%)
0-35 1-100
35-40 100

Flow rate 0.2 mL/min

[MS]

Ionization ESI

Mode MRM

Veterinary Drug Mixture Standard Solution PL-2-1 (each 20μg/ml Methanol Solution)

LC/MS/MS Chromatogram*

00370_img21.png
Peak No. Constituent Monitoring Ions (m/z) Mode Peak No. Constituent Monitoring Ions (m/z) Mode
Precursor Product Precursor Product
1 5-Propylsulfonyl-1H-benzimidazole-2-amine 240.1 133.1 + 13 Sulfachlorpyridazine** 286.2 156.9 +
2 Levamisole** 207.1 180.0 + 14 Sulfadoxine 311.1 155.9 +
3 Thiabendazole 202.2 174.9 + 15 Sulfamethoxazole 254.1 156.0 +
4 Trimethoprim 291.2 230.0 + 16 Ethopabate 238.3 136.0 +
5 Sulfadiazine 251.1 155.9 + 17 Sulfadimethoxine 311.1 156.0 +
6 Ormetoprim 275.2 123.1 + 18 Sulfaquinoxaline** 301.1 156.0 +
7 Sulfathiazole 256.1 155.9 + 19 β-Trenbolone 271.2 199.0 +
8 Sulfapyridine 250.1 156.0 + 20 α-Trenbolone 271.2 199.0 +
9 Sulfamerazine 265.1 92.1 + 21 Melengestrol Acetate 397.3 279.0 +
10 Sulfadimidine 279.1 92.1 + 22 Thiamphenicol 356.1 185.1
11 Sulfamethoxypyridazine 281.1 156.1 + 23 Zeranol 321.3 277.4
12 Sulfamonomethoxine 281.1 156.0 + 24 Sulfanitran 334.0 136.1
  • *Analysis conditions, charts, and detected ions are reference data. It is not the data to guarantee the pesticide mixed standard solution.
  • **The preparation concentration is converted to 20 µg/mL as a free base.

Analysis conditions

[ Instrument ]

Shimadzu LCMS-8040

[HPLC]

Column Wakopak® Wakosil-Ⅱ 3C18HG 3.0 × 150mm

Column temperature 40 ℃

Eluent A) 0.1% HCOOH in H2O, B) 0.1% HCOOH in CH3CN

Gradient

Time (min) B conc. (%)
0-35 1-100
35-40 100

Flow rate 0.2 mL/min

[MS]

Ionization ESI

Mode MRM

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Mixture Standard of Pesticides

Veterinary Drug Mixture Standard Solutions

Author: T. Miura

For research use or further manufacturing use only. Not for use in diagnostic procedures.

Product content may differ from the actual image due to minor specification changes etc.

If the revision of product standards and packaging standards has been made, there is a case where the actual product specifications and images are different.

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